Chemistry
502 - Instrumental Methods of
Analysis – Spring 2008
Qualitative
and/or quantitative methods of chemical analysis for organic, biochemical, and
inorganic compounds fall into two categories, classical (or wet) methods
and instrumental methods. Chemistry 313/314 surveyed some classical
methods of analysis (titration, gravimetric, and volumetric analysis) and some
instrumental methods of analysis (chromatography, spectroscopy &
electrochemistry). Although there is not always a clear barrier between the
two, the primary difference arises from the type of physical property used to
provide information. Classical methods often rely on reactivity or physical
properties such as solubility, color, melting and/or boiling points, odors, or
refractive indices for qualitative information, while gravimetric, volumetric,
and titrimetric measurements provide the quantitative information. Classical methods for the separation of
mixtures are mainly solvent extractions and distillations. Instrumental methods
of analysis typically utilize other physical properties such as absorption or
emission of light, mass-to-charge ratio, electrode potential, current, or
charge measured with modern sophisticated electronic devices. Separations are carried out by more efficient
chromatography and electrophoresis methods.
Instrumental
methods of analysis certainly extend well beyond the chemistry lab. These
instruments are found in biotechnology, environmental, geological, material
development, forensic, medical, nutritional, and industrial labs.
Unfortunately, some scientists view and utilize these instruments as
"black boxes". The term implies a device in which the scientist
places a sample and somehow a number is generated that influences the
scientist’s decision-making process. It should be apparent that this approach
could be dangerous, as the old saying "Garbage In/Garbage Out" is
often true. As such any scientist using sophisticated instrumental equipment
needs at least a basic understanding of how these devices are designed to work.
Instrumental
Methods of Analysis is a broad
subject, but the methods are generally categorized as spectroscopic,
electrochemical, or chromatographic. We
will essentially take the cover off the "black box" and see how these
instruments are constructed and measurements made from the underlying chemical
and physical properties of the substance.
Quantitative problem solving will be utilized as a means to demonstrate
physical principles applied in the design and performance of instruments.
The
goal of this course is not to make you an "expert" on each type of
instrumentation encountered, but rather to introduce and educate you to the
many types of instruments available for chemical analysis and the type(s) of
information these instruments provide. It is my hope that you will then expand
your knowledge of the instruments you come into contact with during your
scientific career, thereby avoiding the "black box" problem.
Specific
Course Objectives:
By
the end of this course, you should:
- Have an
understanding of how chemical and physical properties of substances are
used in the design and construction of modern sophisticated
instrumentation used in chemical analysis
- Have a broad
knowledge of the types of instrumentation generally available and the
information provided by each
- Understand the
advantages, disadvantages, and limitations of different instruments used
for similar types of analyses
- Use rigorous
mathematical methods for evaluating instrument performance
Time/Location:
12:30 - 1:45 TR / Sims 302
Professor:
Dr. C. Calloway callowayc@winthrop.edu
Office:
312-B Sims Hall; 323-4945
Office
Hours: TRF 8:30 - 10:30
a.m. {and other times by appointment.}
Textbook:
Skoog, D.A., Holler, F.J., Crouch, S.R. Principles of Instrumental Analysis, 6thedition.
Grading/Evaluation:
Note: Since all graded work (including homework to
be collected, quizzes, papers, mid-term examinations, final examination,
research proposals, laboratory results and reports, etc.) are used in the
determination of academic progress, no collaboration on such work is permitted unless
the instructor explicitly indicates that some specific degree of collaboration
is allowed. This statement is not intended to discourage students from studying
together, seeking help from the instructor, or working together on assignments
that are not to be collected. These
activities are encouraged.
Grades in this course will be determined from three
sources, as follows:
- Homework (20%):
Periodically, homework problems will be assigned, from the textbook or as
handouts, and collected. Due dates given for each assignment are the final
date each assignment will be accepted.
- Mid-term
Exams (60%): There will be 4 exams given during the term covering the
topics listed below. Make sure
to bring a pencil and calculator to the exam. No make-up exams will be
given, except under extreme conditions.
If an exam is missed with a valid excuse, as determined by the
instructor, the remaining exams will be averaged. The exams are scheduled as follows:
- Exam
1: February 7
- Exam
2: February 28
- Exam
3: April 3
- Exam
4: April 28
- Final Examination:
20% {Tuesday, May 6/11:30 a.m.
– 2:00 p.m.} There will be a cumulative final examination given during
exam week. If you score higher on the final exam than your lowest mid-term
exam, the final exam grade will replace the lowest exam grade, before
averaging.
Letter
grades will be assigned as follows:
94 - 100%: A 90-93%: A- 86-89%: B+ 82-85%: B 78-81%: B-
74-77%: C+ 70-73%: C 66-69%: C- 62-65%: D+ 58-61%: D
55-57%: D-
Menu
of Topics:
- Analytical Figures
of Merit, Basic Electronics,
Signal-to-Noise Theory (Ch.
1,2,3A-C, and 5)
Exam 1
- Spectroscopic
Instrument Design - (Ch.
6,7)
- Molecular
Electronic and Vibrational Spectroscopy (Ch. 13, 15, 16, 18)
Exam 2
- Nuclear Magnetic
Resonance Spectroscopy- (Ch. 19)
- Atomic and Molecular Mass
Spectrometry (Ch.
11,20)
- Surface Analysis (Ch.
21)
Exam 3
- Electro-analytical
Chemistry (Ch. 23-25)
- Advanced
Separations (Ch. 26, 29,30)
Exam 4
Chapter Competencies
Old Exam 1
Old Exam 2
Students
with Disabilities: If
you have a disability and need classroom accommodations, please contact Services
for Students with Disabilities, at 323-3290, as soon as possible. Once you have your “Professor Notification
Form”, please notify me so that I am aware of your accommodations well before
the first test or assignment.
My
advice, to help you succeed in this endeavor:
- Read your textbook.
- Be sure you know
how to do mean, standard deviation, and linear regression on your
calculator.
- Stay ahead of the
lectures in your reading.
- Work the homework
problems by yourself, without any aid.
- Don’t fall behind.
- Wear sunscreen.
- Read your textbook.
- Floss at least once
a day.
- Talk to your
professor, especially if you are confused.
- Get a good night’s
rest.
- Read your textbook.
- Sing occasionally.
- Above all, read
your textbook.